Objectives:

o development of quantitative laboratory skills

o introduction to modern analytical science

Approach:

o solve a series of chemical analysis problems with various techniques and instruments

o certify laboratory instruments and standards

o maintain laboratory records in compliance with Good Laboratory Practice Guidelines

Schedule:

Weeks 1-4

- Perform Basic Set of three fundamental experiments (Series A)

- Begin Calibration and Materials Certification Procedures (Series C & D)

Weeks 5-15

Three parallel activities will be sustained:

- Perform a series of quantitative studies (Series B)

- Calibration of laboratory instruments (Series C)

- Certification of laboratory standard materials (Series D)

(Each student will perform each experiment in the B-series.)

(Each student will perform an assigned set from the C- & D-series

certification and calibration procedures (see next page))

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A. Basic Quantitative Techniques

(A.1) Gravimetric determination of chloride in a solid mixture

(NOTE: The material analyzed by each student in this

experiment will be used as a reference material in a

subsequent experiment; see B.2)

(A.2) Determination of Mg/Ca mixtures by EDTA titration

(NOTE: The skills learned in this experiment will be used

repeatedly during the semester for certification of metal

solution standards; see D.1, D.2.)

Determination of Mn in Steel

(NOTE: Least squares regression analysis will be used for this

and later experiments, to construct calibration curves.

B. Quantitative Analytical Studies

The following experiments will be conducted simultaneously, with each student signing up for available time on required equipment.

(Due dates for results will be indicated by the Lab Instructor.)

(B.1) Titration of a polyprotic acid (phosphate)

(NOTE: Calibration of the pH electrode (assignment C.1) is a required

part of this experiment.)

(B.2) Potentiometric Determination of Cl in Solid Mixtures with

varying chloride salt particle sizes

(NOTE: Calibration of the chloride electrode (assignment C.1) is a required

part of this experiment. The chloride standard is that certified in A.1.)

(B.3) Voltammetric Determination of Vitamin C in Fruit Drink

(B.4) Multi-element Voltammetric Trace Analysis of Heavy Metal Ions in

Seawater (Optional)

(B.5) Determination of Polyaromatic Hydrocarbons in a Mixture

using High Performance Liquid Chromatography (HPLC)

Using Gradient HPLC (Spectraphysics System) (Optional)

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C. Instrument Calibration Procedures

(Do C.1 and any one of C.2 to C.5)

(C.1) pH Electrodes and Chloride Electrodes

(C.2) Spectrophotometer

(C.3) Voltammetric Analyzer

(C.4) Atomic Absorption Spectrometer

(C.5) HPLC System

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D. Certification of Laboratory Standard Reagents

(Do D.1 and any one solution from D.2, D.3)

Each laboratory standard reagent will be certified periodically, as assigned, by individual students, using prescribed procedures.

(D.1) Chloride solid mixed salt (for potentiometric determination) [From A.1]

(Each student certifies the composition of a different reference material as part of

Experiment A.1)

(D.2) Mn²⁺, Co²⁺, Zn²⁺ (for calibration of spectrometers) [EDTA titrations]